CN111057881B - Method for recovering tungsten from purification slag - Google Patents
Method for recovering tungsten from purification slag Download PDFInfo
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- CN111057881B CN111057881B CN201911414075.3A CN201911414075A CN111057881B CN 111057881 B CN111057881 B CN 111057881B CN 201911414075 A CN201911414075 A CN 201911414075A CN 111057881 B CN111057881 B CN 111057881B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/11—Removing sulfur, phosphorus or arsenic other than by roasting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Environmental & Geological Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for recovering tungsten from purification slag, which is characterized by comprising the following steps: immersing the purified slag and soda in an aqueous solution, mixing, boiling, performing solid-liquid separation, and recovering to obtain a sodium tungstate solution; wherein the molar weight ratio of the tungsten content in the purification slag to the soda is 1: (2.5-3.5). According to the method, the purification slag is soaked and boiled by adding the soda, so that the tungsten, silicon, phosphorus and other elements in the purification slag are effectively separated, the obtained sodium tungstate solution can be used for preparing ammonium paratungstate after being purified, and the overall recovery rate of the tungsten is improved.
Description
Technical Field
The invention relates to a method for treating waste residue containing tungsten, in particular to a method for recovering tungsten from purified residue.
Background
Tungsten has the characteristics of high density, high hardness, high melting point and the like, is widely applied to the fields of illumination, metallurgy, hard alloy cutters, military industry and the like, and is an important metal material with strategic significance. Although the reserves, the yields and the export of the tungsten mineral resources in China are the first in the world, in recent years, due to the fact that the natural tungsten mineral resources are rapidly reduced due to over-exploitation of the tungsten mineral resources, sustainable development is seriously affected, and therefore secondary utilization of the tungsten resources is vigorously developed to replace exploitation of raw ores by recycling, and the method becomes a direction needing to be vigorously promoted at present.
Because the hard alloy has higher tungsten grade, the method has higher attention to the recovery and extraction of tungsten in the waste hard alloy at present. At present, a method for recovering tungsten from waste hard alloy in an ammonium paratungstate mode is disclosed, wherein a crude sodium tungstate solution is obtained by cobalt dissolution, oxidation and alkaline leaching, other impurity elements in the crude sodium tungstate are separated, and finally, ammonium paratungstate is obtained by crystallization. In the practical production and application process, after the crude sodium tungstate solution is obtained by alkaline leaching, the solution is usually purified to remove impurities, and elements such as silicon, phosphorus and the like contained in the solution are removed; because excessive magnesium sulfate solution is usually adopted to remove silicon and phosphorus in the purification and impurity removal process, part of magnesium tungstate can be generated in the purification slag obtained after purification and impurity removal, so that part of tungsten can be lost from the purification slag, and the recovery amount of tungsten is reduced. Therefore, it is necessary to provide a method for recovering tungsten from the purification slag, which is used for reducing the loss of tungsten.
Disclosure of Invention
The invention aims to provide a method for recovering tungsten from purification slag, which is used for solving the problem that tungsten contained in the purification slag is not utilized in the prior art.
In order to solve the technical problem, the invention provides a method for recovering tungsten from purification slag, which comprises the following steps: immersing the purified slag and soda in an aqueous solution, mixing, boiling, performing solid-liquid separation, and recovering to obtain a sodium tungstate solution; wherein the molar weight ratio of the tungsten content to the soda in the purification slag is 1: (2.5-3.5).
Wherein when the purification slag and the soda are immersed in water, the solid-liquid mass ratio is 1: 4.
Wherein in the step of solid-liquid separation after mixing and boiling, the leaching temperature is 80-240 ℃.
Wherein in the step of solid-liquid separation after mixing and boiling, the leaching time is 2.5-3.5 h.
Wherein, the recovered sodium tungstate solution is used for preparing ammonium paratungstate after being purified.
The invention has the beneficial effects that: the method is characterized in that the purification slag is soaked and boiled by adding soda, so that tungsten in the purification slag is effectively separated from elements such as silicon, phosphorus and the like, and the obtained sodium tungstate solution can be used for preparing ammonium paratungstate after purification treatment, so that the overall recovery rate of tungsten is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The method for recovering tungsten from purification slag comprises the following steps: immersing the purified slag and soda in an aqueous solution, mixing, boiling, performing solid-liquid separation, and recovering to obtain a sodium tungstate solution; and purifying the recovered sodium tungstate solution to prepare ammonium paratungstate.
In the present embodiment, it is preferable that the molar weight ratio of the tungsten content to the soda in the purification residue is 1: (2.5-3.5), when the purification slag and the soda are immersed in water, the solid-liquid mass ratio is 1: 4; and in the step of solid-liquid separation after mixing and boiling, the leaching temperature is 80-240 ℃, and the leaching time is 2.5-3.5 h.
Specifically, the reaction mechanism of the method for recovering tungsten from the purification slag is explained in detail. The purification slag mentioned in the invention is slag generated after the purification and impurity removal of a crude sodium tungstate solution in the process flow of preparing ammonium paratungstate, tungsten in the purification slag mainly exists in the form of magnesium tungstate, and meanwhile, the purification slag also contains silicon, phosphorus and other impurity elements; when a proper amount of soda is added for digestion, magnesium tungstate and sodium carbonate react to generate magnesium carbonate and sodium tungstate, and tungsten element exists in the solution in the form of sodium tungstate, so that slag is separated from the tungsten element; because the phosphorus and silicon impurities in the purification slag mainly exist in the forms of magnesium phosphate and magnesium silicate, the solubility product constants of the phosphorus and silicon impurities are small and are both smaller than the solubility of magnesium carbonate, when sodium carbonate reacts with magnesium tungstate, the sodium carbonate does not basically react with the magnesium phosphate and the magnesium silicate, so that the tendency that the phosphorus and silicon impurities enter a solution is small, the solution after the reaction is mainly sodium tungstate, and the separation of tungsten and other impurity elements in the purification slag is realized.
The method for recovering tungsten from the purification slag of the present invention is described in detail by the following embodiments, wherein the purification slag selected in the following embodiments is a sample with the same components, and the mass percentage of some components in the purification slagThe number is as follows: WO324.83% of P, 0.34% of SiO20.175 percent of Mg and 13.97 percent of Mg.
Example 1
Immersing 200g of purified slag and 60g of soda in water to ensure that the theoretical molar ratio of magnesium tungstate in the purified slag to the added sodium carbonate is 1:1, controlling the added water to ensure that the solid-liquid ratio before digestion is 1:4, performing digestion at 100 ℃ for 3 hours under normal pressure, and recovering the sodium tungstate solution after solid-liquid separation. The test shows that the recovery rate of tungsten is 91.2 percent, and the leaching residue contains tungsten (WO)3Calculated) the mass percent is 3.08%; the recovered sodium tungstate solution contains 0.01g/L of phosphorus and Silicon (SiO)2Calculated) the content was 1.2 g/L.
Example 2
Immersing 200g of purification slag and 72g of soda in water to ensure that the theoretical molar ratio of magnesium tungstate in the purification slag to the added sodium carbonate is 1:1, controlling the added water to ensure that the solid-liquid ratio before digestion is 1:4, performing high-pressure digestion at 150 ℃ for 2.5h, and recovering after solid-liquid separation to obtain a sodium tungstate solution. Tests show that the recovery rate of tungsten is 95.28%, and the leached residue contains tungsten (WO)3Calculated) the mass percent is 1.76 percent; the recovered sodium tungstate solution contains 0.23g/L of phosphorus and Silicon (SiO)2Calculated) the content was 1.34 g/L.
It can be seen from the above examples 1 and 2 that the recovery rates of the tungsten recovered by the above immersion cooking method are both greater than 90%, and the tungsten element in the purification slag can be well recycled, thereby improving the overall recovery rate of tungsten in the process of recovering and preparing ammonium paratungstate; meanwhile, the sodium tungstate solution obtained after immersion and boiling contains extremely low content of other elements, so that the purity of the sodium tungstate is improved, and the sodium tungstate solution can be applied to subsequent preparation of ammonium paratungstate after simple purification treatment.
The method is characterized in that the purification slag is soaked and boiled by adding soda, so that tungsten in the purification slag is effectively separated from elements such as silicon, phosphorus and the like, and the obtained sodium tungstate solution can be used for preparing ammonium paratungstate after purification treatment, so that the overall recovery rate of tungsten is improved.
It should be noted that the above embodiments belong to the same inventive concept, and the description of each embodiment has a different emphasis, and reference may be made to the description in other embodiments where the description in individual embodiments is not detailed.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (2)
1. A method for recovering tungsten from purification slag is characterized by comprising the following steps: immersing the purified slag and soda in an aqueous solution, mixing, boiling, performing solid-liquid separation, and recovering to obtain a sodium tungstate solution;
wherein the molar weight ratio of the tungsten content in the purification slag to the soda is 1: (2.5-3.5), wherein impurities of phosphorus and silicon in the purification slag exist in the forms of magnesium phosphate and magnesium silicate;
in the step of solid-liquid separation after mixing and boiling, the leaching temperature is 80-240 ℃, and the leaching time is 2.5-3.5 h;
and purifying the recovered sodium tungstate solution for preparing ammonium paratungstate.
2. The method for recovering tungsten from the purification slag as claimed in claim 1, wherein the purification slag and the soda are immersed in water at a solid-liquid mass ratio of 1: 4.
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| CN110512095B (en) * | 2019-08-21 | 2020-07-10 | 长沙矿冶研究院有限责任公司 | Method for extracting and stabilizing arsenic from tungsten metallurgy phosphorus arsenic slag |
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